公开(公告)号：US4769494A

公开(公告)日：1988-09-06

申请号：US11009

申请日：1987-02-05

申请人： Motomasa Ohsu ,  Koichi Kamemoto ,  Manabu Yahata ,  Tooru Tokumaru ,  Takeshi Hioki ,  Hiroshi Ueda

发明人： Motomasa Ohsu ,  Koichi Kamemoto ,  Manabu Yahata ,  Tooru Tokumaru ,  Takeshi Hioki ,  Hiroshi Ueda

IPC分类号： C07F9/20 ,  C07F9/02

CPC分类号： C07F9/20

摘要： A continuous process for producing O,O-di-lower alkylchlorothiophosphate very important as an intermediate for organo-phosphate series agricultural chemicals which comprises continuously reacting phosphorus sulfochloride with a lower alcohol in the presence of caustic soda according to a multi-stage reaction form comprising from 3 to 8 stages in which the following conditions are satisfied:(1) The amounts of caustic soda and a lower alcohol used shall be from 2 to 2.2 moles and 10 moles or more, respectively, based on 1 mole of phosphorus sulfochloride.(2) Caustic soda, water and the lower alcohol shall be used as a caustic soda/water/lower alcohol solution, and besides the caustic soda concentration of the aqueous caustic soda in said solution shall be from 30.0 to 99.5 wt.%.(3) To the 1st reaction stage shall be continuously supplied the whole amount of phosphorus sulfochloride required and from 45 to 85 wt.% each of the amounts of caustic soda and the lower alcohol required; and to the 2nd and subsequent reaction stages shall be continuously supplied the residual caustic soda and lower alcohol in divided portions so that the substantial amounts supplied become successively small toward the final reaction stage.(4) The temperature of the reaction system shall be -5.degree. C. or lower.(5) The residence time in the reaction system shall be within 4 hours.

摘要翻译： 一种用于生产作为有机磷酸酯系农药的中间体非常重要的O，O-二低级烷基氯硫代磷酸酯的连续方法，其包括在苛性钠存在下，根据多阶段反应形式连续地使磷酰氯与低级醇反应，包括 从3到8个阶段，其中满足以下条件：（1）基于1摩尔磷酰氯，苛性钠和低级醇的用量分别为2至2.2摩尔和10摩尔或更多。 （2）苛性钠，水和低级醇应用作苛性钠/水/低级醇溶液，除了所述溶液中的苛性钠水溶液的苛性钠浓度外还应为30.0至99.5重量％。 （3）向第一反应阶段连续供应所需的全部硫磺磷酸盐和每一种苛性钠和所需的低级醇的45至85重量％; 并且连续向第二和随后的反应阶段连续地供应残留的苛性钠和低级醇，使得所供应的实质量向着最终反应阶段依次小。 （4）反应体系的温度应在-5℃以下。 （5）反应体系中的停留时间应在4小时内。